惰性熔融红外吸收/热导法测定TiCN原料粉末中氧和氮
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摘要
通过惰性熔融红外吸收/热导法建立了TiCN原始粉末中氧和氮质量分数的测定方法。测定实验表明,采用镍+锡作为助熔剂,分析功率在5500 W,称样量应该控制在0.03～0.05 g,样品熔融良好,释放完全。选用钛合金作为氧的校准曲线,选用钒氮合金作为氮的校正曲线,考察了TiCN原始粉末的精密度,氧的相对标准偏差为1%左右,氮的相对标准偏差为1%左右。回收率实验表明,氧的回收率在99%～103%之间,氮的回收率在98%～100%之间,分析结果精度和准确度令人满意,满足实际生产要求。
The determination method of oxygen and nitrogen contents by mass in TiCN raw material powders was established by inert fusion infrared absorption/thermal conductivity method. Ni and Sn were used as the fluxes, the analysis power was 5500 W, and the sample mass should be controlled at 0.03～0.05 g. The sample was well melted and released completely. Titanium alloy was selected as the calibration curve of oxygen, the vanadium nitrogen alloy was selected as the calibration curve of nitrogen, and the precision of TiCN powders was investigated. In the results, the relative standard deviation of oxygen is about 1%, and the relative standard deviation of nitrogen is about 1%. The recovery experiment shows that the recovery rate of oxygen is between 99% and 103%, and that of nitrogen is between 98% and 100%, meeting the actual production requirements.
The determination method of oxygen and nitrogen contents by mass in TiCN raw material powders was established by inert fusion infrared absorption/thermal conductivity method. Ni and Sn were used as the fluxes, the analysis power was 5500 W, and the sample mass should be controlled at 0.03～0.05 g. The sample was well melted and released completely. Titanium alloy was selected as the calibration curve of oxygen, the vanadium nitrogen alloy was selected as the calibration curve of nitrogen, and the precision of TiCN powders was investigated. In the results, the relative standard deviation of oxygen is about 1%, and the relative standard deviation of nitrogen is about 1%. The recovery experiment shows that the recovery rate of oxygen is between 99% and 103%, and that of nitrogen is between 98% and 100%, meeting the actual production requirements.
引文
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[15]Lin W Q,He Y N.Determination of oxygen and nitrogen in ceramic material AlN and TiCN.J Iron Steel Res,1992,4(3):87(林文泉,何永年.陶瓷材料AlN及TiCN中氧、氮的测定.钢铁研究学报,1992,4(3):87)
[2]Yan D K,Zhang H A,Yi J Y,et al.Study on preparation and microwave sintering process of ultra-fine TiCN matrix cermet.Hot Working Technol,2010,39(20):73(严迪科,张厚安,易继勇,等.超细TiCN基金属陶瓷的制备及其微波烧结工艺研究.热加工工艺,2010,39(20):73)
[3]Ma L L,Liu B,Yu Q X,et al.Development and application of metal ceramic cutting tool materials.Aeronaut Manuf Technol,2008(7):100(马丽林,刘滨,于启勋,等.金属陶瓷刀具材料的发展和应用.航空制造技术,2008(7):100)
[4]Deng L C,Hu X P.Determination of oxygen and nitrogen in the AlN.Cemented Carbide,1997,14(3):181(邓隆长,胡新平.AlN中氧和氮的测定.硬质合金,1997,14(3):181)
[5]Wang H T,Li H.Research progress on the sintering technology and properties of fine-grained Ti(C,N)cermets.Powder Metall Ind,2015,25(5):66(王洪涛,李宏.细晶Ti(C,N)金属陶瓷烧结技术与性能研究进展.粉末冶金工业,2015,25(5):66)
[6]He C X,Xia Z H,Wang Y M,et al.Study of Ti(C,N)-based metal ceramic.Chin J Rare Met,1999,23(1):4(贺从训,夏志华,汪有明,等.Ti(C,N)基金属陶瓷的研究.稀有金属,1999,23(1):4)
[7]Han C L,Liu N,Fan G N,et al.Effects of starting powders size on the microstructures of TiCN-based cermets.Powder Metall Technol,2006,24(4):251(韩成良,刘宁,范广能,等.原料粉末粒度对Ti CN基金属陶瓷微观组织的影响.粉末冶金技术,2006,24(4):251)
[8]Xiong J,Zhang Y K,Shen B L,et al.The preparation and performance of superfine TiCN cermet.Powder Metall Technol,2003,21(2):92(熊继,张亚昆,沈保罗,等.超细TiCN金属陶瓷的制备及性能.粉末冶金技术,2003,21(2):92)
[9]Tang S W,Zhang H A,Yan J H,et al.Research on preparing ultra-fine grain TiCN matrix cermets by vacuum microwave sintering.Powder Metall Technol,2010,28(3):220(唐思文,张厚安,颜建辉,等.真空微波烧结制备TiCN基金属陶瓷.粉末冶金技术,2010,28(3):220)
[10]Xiong H W,Wen Y,Gan X P,et al.Influence of coarse TiCN content on the morphology and mechanical properties of ultrafine TiCN-based cermets.Mater Sci Eng A,2017,682:648
[11]Chen M H,Shen R M,Ai X T.State analysis of oxygen in ultrafine nitride and carbide powders.J Iron Steel Res,1996,8(1):45(陈名浩,沈汝美,艾星涛.氮碳化合物超细粉中氧的状态分析.钢铁研究学报,1996,8(1):45)
[12]Zhang Y M,Zhu L H,Ban Z G,et al.Effect of oxygen addition on microstructure and properties of TiCN coating deposited by chemical vapor deposition.Cemented Carbide,2012,29(2):66(张雨萌,朱丽慧,班志刚,等.氧的掺入对化学气相沉积TiCN涂层的影响.硬质合金,2012,29(2):66)
[13]Zhang Z X.Determination of nitrogen in nitride.Rare Met Mater Eng,1994,23(2):74(张之翔.氮化物材料中氮的测定.稀有金属材料与工程,1994,23(2):74)
[14]He Y.Determination of nitrogen content in Ti CN-based cermet and its raw material by alkaline distillation.Powder Metall Technol,2011,29(1):41(何英.碱蒸馏分离-酸碱滴定法测定TiCN基合金及其原料中氮.粉末冶金技术,2011,29(1):41)
[15]Lin W Q,He Y N.Determination of oxygen and nitrogen in ceramic material AlN and TiCN.J Iron Steel Res,1992,4(3):87(林文泉,何永年.陶瓷材料AlN及TiCN中氧、氮的测定.钢铁研究学报,1992,4(3):87)
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